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Method of forming a βSiAlON by spark plasma sintering

a technology of sintering and sialon, applied in the direction of sialons, nitrogen and non-metal compounds, etc., can solve the problem of inability to achieve the complete densification of the sisub>3/sub>nsub>4/sub>

Active Publication Date: 2022-10-25
KING FAHD UNIVERSITY OF PETROLEUM AND MINERALS
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the presence of covalent bonds between Si and N atoms, complete densification of the Si3N4 cannot be easily achieved.

Method used

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  • Method of forming a βSiAlON by spark plasma sintering
  • Method of forming a βSiAlON by spark plasma sintering
  • Method of forming a βSiAlON by spark plasma sintering

Examples

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example 1

Experimental Procedure

[0092]Two Si3N4 powders with different structures and sizes (β-Si3N4, particle size ˜44 μm, Sigma-Aldrich, Germany; amorphous Si3N4, particle size 20-40 nm, Chempur, Germany) were used as a starting powder. Other additives incorporated were AlN (size=50 nm, Chempur, Germany), Al2O3 (size2 (10-20 nm, Sigma-Aldrich, Germany) to synthesize β-Sialon (general formula of Si6−ZAlZOZN8−Z). In the following text, sample IDs (A-ZX-T or B-ZX-T) starting with “A” represent samples synthesized using amorphous Si3N4, whereas those starting with “B” represent samples synthesized using β-Si3N4. Moreover, “X” having the value of 1, 2, or 3, represents the value of the variable Z in the general formula of β-Sialon, whereas “T” represents the synthesis temperature in degrees Celsius. The schematic shown in FIG. 1 exhibits the selected compositions (marked by centrally-located circles) used in the present study. The weight percentage of the starting powders along with their respec...

example 2

Results and Discussion≤Characterization of as-Received Powder Precursors

[0098]FESEM micrographs of the as-received nanosized amorphous Si3N4 at different magnifications are shown in FIGS. 3A-3B. The micrographs revealed that the particle size of the powder is uniform. Further investigation by TEM confirmed that the particle sizes of the amorphous Si3N4 and the SiO2 are in the ranges 20-40 nm and 10-20 nm, respectively (FIGS. 4A-4D). The superimposed selected-area electron diffraction (SAED) pattern confirms the presence of diffused rings and the amorphous nature of the as-received nanosized Si3N4 and SiO2 powders, as indicated by the absence of lattice fringes in the high-resolution TEM images (FIGS. 4B and 4D, respectively).

[0099]High-temperature XRD scans were performed to analyse the phase evolution of the starting powder mixtures at different temperatures. The XRD pattern in FIG. 5A is for the starting powder mixture containing nanosized amorphous Si3N4 (A-Z1). The low-intensity...

example 3

Results and Discussion—Density, Mechanical Properties, and Thermal Properties of the SPSed Samples

[0104]Table 3 shows the density, Vickers hardness (HV10), fracture toughness (KIc), thermal expansion coefficient values, and XRD phases for the β-Sialon samples (Z=1, 2, and 3) synthesized at 1400, 1500, and 1600° C. using amorphous Si3N4. The density was observed to increase as the synthesis temperature was increased from 1400 to 1600° C. for the same Z value. The Vickers hardness of the samples decreased with increasing synthesis temperature for the same Z values, and the Vickers hardness value decreased with increasing Z value for the same synthesis temperature. Dissolution of the AlN polytype phase at higher temperatures and the formation of coarser and more elongated grains was attributed to the decrease in Vickers hardness. The fracture toughness values were in the range 3.3-4.6 MPa·m1 / 2. The sample with Z=1 and a synthesis temperature of 1500° C. resulted in the highest Vickers ...

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Abstract

A method of making a β-SiAlON is described in involves mixing nanoparticles of AlN, Al2O3, and SiO2 with particles of Si3N4 and spark plasma sintering the mixture. The sintering may be at a temperature of 1450-1600° C. or about 1500° C. The particles of Si3N4 may be nanoparticles comprising amorphous Si3N4, or 25-55 μm diameter microparticles comprising β-Si3N4.

Description

STATEMENT OF ACKNOWLEDGEMENT[0001]This project was prepared with financial support from King Abdulaziz City for Science and Technology (KACST) through the Science & Technology Unit at King Fahd University of Petroleum & Minerals (KFUPM): Project no. 12-ADV2411-04 as part of the National Science, Technology and Innovation Plan.BACKGROUND OF THE INVENTIONTechnical Field[0002]The present invention relates to a method of forming a β-SiAlON by spark plasma sintering a precursor powder mixture.Description of the Related Art[0003]The “background” description provided herein is for the purpose of generally presenting the context of the disclosure. Work of the presently named inventors, to the extent it is described in this background section, as well as aspects of the description which may not otherwise qualify as prior art at the lime of filing, are neither expressly or impliedly admitted as prior art against the present invention.[0004]Ceramic materials have been widely used as tools unde...

Claims

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Application Information

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Patent Type & Authority Patents(United States)
IPC IPC(8): C01B21/082C04B35/597C04B35/64C04B35/645
CPCC01B21/0826C04B35/597C04B35/64C04B35/645C01P2002/72C01P2004/03C01P2004/04C01P2004/64C01P2006/10C01P2006/32C01P2006/80
Inventor HAKEEM, ABBAS SAEEDUL-HAMID, ANWARMURAZA, OKIEHSAN, MUHAMMAD ALI
Owner KING FAHD UNIVERSITY OF PETROLEUM AND MINERALS
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